CN101629004A - Preparation method of rare earth modified nano TiO2/polytetrafluoroethylene composite - Google Patents
Preparation method of rare earth modified nano TiO2/polytetrafluoroethylene composite Download PDFInfo
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- CN101629004A CN101629004A CN200910055617A CN200910055617A CN101629004A CN 101629004 A CN101629004 A CN 101629004A CN 200910055617 A CN200910055617 A CN 200910055617A CN 200910055617 A CN200910055617 A CN 200910055617A CN 101629004 A CN101629004 A CN 101629004A
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- tio
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Abstract
The invention relates to a preparation method of a rare earth modified nano TiO2/polytetrafluoroethylene composite, comprising the following steps: first adopting a rare earth modifier at room temperature to carry out surface modification treatment on the nano TiO2, then placing the treated nano TiO2 into a ball mill to undergo ball milling, mechanically blending the nano TiO2 undergoing ball milling with polytetrafluoroethylene powder, controlling the weight percent of the nano TiO2 to be 3-15% of the blended powder, then placing the blended powder into a die to be formed by pressing and preparing the composite through high temperature sintering, wherein, the rare earth modifier is prepared by rare earth compounds, ethanol, ethylene diamine tetraacetic acid, ammonium chloride, nitric acid and urea. The method is simple in process, low in cost and free of environmental pollution, and the prepared rare earth modified nano TiO2/polytetrafluoroethylene composite enjoys good mechanical property and tribological property.
Description
Technical field
The present invention relates to a kind of composite material and preparation method thereof, relate in particular to a kind of rare earth modified nano TiO
2/ ptfe composite preparation method adopts the nano-TiO through rare-earth modifier for treatment
2Filled polytetrafluoroethylene prepares matrix material, to obtain than higher interface binding power the mechanical property of raising teflon resin matrix, and then the practical engineering application value of raising matrix material.
Background technology
Tetrafluoroethylene is to be rich in one of antifriction material of potentiality most, the self-lubricating property of have that moulding process is simple, cost is low, recyclable repeated use, frictional coefficient are extremely low, good and the distinct advantages such as use temperature scope of broad.But, because tetrafluoroethylene molecule interchain attraction is less, cause that bad mechanical property, linear expansivity are big, poor thermal conductivity, abrasion loss be big, be unsuitable for doing separately high-abrasive material and use.Usually in tetrafluoroethylene, add filler and carry out filling-modifiedly, be prepared into ptfe composite,, obtain good wear resistance and high strength, high rigidity and dimensional stability in the hope of when keeping its low-friction coefficient.
TiO
2Being commonly called as titanium white, is that titanium is one of most important product, also is a kind of important chemical and environmentally conscious materials.Nano-TiO
2Have that particle diameter is little, specific surface area is big, surfactivity is high, magnetic is strong, photochemical catalysis and advantage such as absorptive character are good, heat conductance is good, and have super hydrophilic interaction and antibacterial.Owing to have these novel characteristics, TiO
2Application in plastics also gives body material many new performances except that strengthening toughening effect.With nano-TiO
2Be dispersed in the polymeric matrix with nano-scale, can obtain nano-TiO
2Plastics.In order to improve nano-TiO
2Dispersed and increase itself and the bonding force of polymer interface, need carry out modification to its surface, to reduce its surperficial energy state, make in the reasonable matrix material that be applied to polymkeric substance of its energy and go.Adopt nano-TiO through rare-earth modifier for treatment
2Filled polytetrafluoroethylene can obtain having the brand-new hi-tech matrix material of the excellent properties that general matrix material do not have, but not see have correlation technique openly to report at present.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of rare earth modified nano TiO is provided
2/ ptfe composite preparation method, it is simple to have technology, and the characteristics of low-cost high-efficiency can well be improved nano-TiO
2With the interface binding power of poly tetrafluoro ethylene matrix, thus the over-all properties of raising matrix material.
For realizing such purpose, in the technical scheme of the present invention, at room temperature adopt rare-earth modifier to nano-TiO earlier
2Carry out surface modification treatment, the nano-TiO after will handling again
2Put into the ball mill ball milling, then with the nano-TiO behind the ball milling
2Mechanical blending is carried out according to a certain percentage with tetrafluoroethylene in the oven dry back, the control nano-TiO
2Weight percent be 3～15% of mixed powder, again mixed powder is put into mould compression moulding, obtain rare earth modified nano TiO through high temperature sintering
2/ ptfe composite is made nano-TiO by mechanical workout again
2/ ptfe composite sample or part.Wherein, the component of rare-earth modifier comprises rare earth compound, ethanol, ethylenediamine tetraacetic acid (EDTA), ammonium chloride, nitric acid and urea.
Composite material and preparation method thereof of the present invention is specific as follows:
1, with nano-TiO
2Immerse in the rare-earth modifier and soaked 2～5 hours, filter the back oven dry, obtain nano-TiO through the rare earth surface modification treatment
2The weight percentages of components of described rare-earth modifier is: rare earth compound 0.2～2.3%, ethanol 93.6～99.34%, ethylenediamine tetraacetic acid (EDTA) 0.03～0.7%, ammonium chloride 0.2～1%, nitric acid 0.03～0.6%, urea 0.2～1.8%.
2, the nano-TiO after will handling
2Mix with distilled water, be made into nano-TiO
2Weight percent be 1～10% solution, put into planetary ball mill ball milling 15～65min, rotating speed is 120～550r/min; With the nano-TiO behind the ball milling
2After putting into the abundant oven dry of baking oven, carry out mechanical blending with the tetrafluoroethylene powder, the control nano-TiO
2Weight percent be 3～15% of mixed powder.
3, mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 30～40MPa, and the time is 30～50 minutes, and pressurization and stress-relief process all slowly carry out.
4, the blank with above-mentioned compression moulding takes out gently, puts into muffle furnace, carries out sintering: slowly be warming up to 320～330 ℃ earlier, and then be warming up to 390 ℃ with 30 ℃/hour speed, be incubated 6～7 hours, obtain nano-TiO
2/ ptfe composite.
The nano-TiO that the present invention obtains
2/ ptfe composite can pass through mechanical workout again, makes nano-TiO
2/ ptfe composite sample or part.
Rare earth compound described in the present invention can be Cerium II Chloride, lanthanum trioxide, cerium oxide or Lanthanum trichloride.
Described tetrafluoroethylene comprises with suspension polymerization and through the teflon resin of the broken various trades mark that form of fine powder, as SM021 etc.
The present invention adopts rare-earth modifier, ball mill to handle nano-TiO
2, can improve the interface binding power of matrix material better, improve nano-TiO
2Dispersiveness, thereby improve the tribological property and the mechanical property of matrix material more significantly, and the rare-earth modifier for treatment processing method is simple, cost is low, environmentally safe.Adopt through rare earth surface-treated nano-TiO
2The matrix material that filled polytetrafluoroethylene is made is compared with common similar matrix material, has better mechanical property and tribological property.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described, but do not constitute limitation of the invention.
Embodiment 1
Used starting material comprise: teflon resin, the SM021-F type that ShanghaiChlorine and Alkali Chemical Co Ltd produces.Nano-TiO
2: Haitai Nano Material Co., Ltd., Nanjing, median size is 50～80nm.
1, earlier to nano-TiO
2Carry out pre-treatment, with nano-TiO
2At room temperature immerse in the rare-earth modifier, soaked 3 hours, filter the back oven dry, obtain nano-TiO through the rare earth surface modification treatment
2The weight percentages of components of described rare-earth modifier is: Cerium II Chloride 0.8%, ethanol 96.75%, ethylenediamine tetraacetic acid (EDTA) 0.3%, ammonium chloride 0.6%, nitric acid 0.35%, urea 1.2%.
2, the nano-TiO after will handling
2Mix with distilled water, be made into nano-TiO
2Weight percent be 5% solution, put into planetary ball mill ball milling 40min, rotating speed is 150r/min; With the nano-TiO that obtains behind the ball milling
2The baking oven of putting into 120 ℃ is fully dried, then with tetrafluoroethylene powder and nano-TiO
2Mix, carry out powerful mechanical stirring, in the mixed powder, nano-TiO
2Weight percent be 6.5%, the weight percent of tetrafluoroethylene is 93.5%.
3, mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 40MPa, and the time is 30 minutes, and pressurization and stress-relief process all slowly carry out.
4, the blank with above-mentioned compression moulding takes out gently, puts into muffle furnace, carries out sintering: slowly be warming up to about 330 ℃ earlier, and then be warming up to about 390 ℃ with 30 ℃/hour speed, be incubated 6 hours, obtain nano-TiO
2/ ptfe composite.
With above-mentioned gained nano-TiO
2/ ptfe composite is machined into the matrix material sample of 20mm * 10mm * 10mm, records on the M-2000 friction wear testing machine: frictional coefficient is 0.2, and the specific wear rate is 1.05 * 10-14m3/N.m.
Recording its tensile strength according to the GB1040-79 standard is 36.3MPa.
Recording its flexural strength according to the GB/T9341-2000 standard is 56.3MPa.
Embodiment 2
Used starting material comprise: teflon resin, the SM021-F type that ShanghaiChlorine and Alkali Chemical Co Ltd produces.Nano-TiO
2: Haitai Nano Material Co., Ltd., Nanjing, median size is 50～80nm.
1, earlier to nano-TiO
2Carry out pre-treatment, with nano-TiO
2At room temperature immerse in the rare-earth modifier, soaked 2 hours, filter the back oven dry, obtain nano-TiO through the rare earth surface modification treatment
2The weight percentages of components of described rare-earth modifier is: lanthanum trioxide 1%, ethanol 96.9%, ethylenediamine tetraacetic acid (EDTA) 0.2%, ammonium chloride 0.5%, nitric acid 0.2%, urea 1.2%.
2, the nano-TiO after will handling
2Mix with distilled water, be made into nano-TiO
2Weight percent be 8% solution, put into planetary ball mill ball milling 50min, rotating speed is 230r/min; With the nano-TiO that obtains behind the ball milling
2The baking oven of putting into 120 ℃ is fully dried, then with tetrafluoroethylene powder and nano-TiO
2Mix, carry out powerful mechanical stirring, in the mixed powder, nano-TiO
2Weight percent be 10%, the weight percent of tetrafluoroethylene is 90%.
3, mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 35MPa, and the time is 40 minutes, and pressurization and stress-relief process all slowly carry out.
4, the blank with above-mentioned compression moulding takes out gently, puts into muffle furnace, carries out sintering: slowly be warming up to about 320 ℃ earlier, and then be warming up to about 390 ℃ with 30 ℃/hour speed, be incubated 6 hours, obtain nano-TiO
2/ ptfe composite.
Above-mentioned gained nano TiO 2/ptfe composite is machined into the matrix material sample of 20mm * 10mm * 10mm, and record on the M-2000 friction wear testing machine: frictional coefficient is 0.21, and the specific wear rate is 1.1 * 10-14m3/N.m.
Recording its tensile strength according to the GB1040-79 standard is 33.5MPa.
Recording its flexural strength according to the GB/T9341-2000 standard is 52.8MPa.
Embodiment 3
Used starting material comprise: teflon resin, the SM021-F type that ShanghaiChlorine and Alkali Chemical Co Ltd produces.Nano-TiO
2: Haitai Nano Material Co., Ltd., Nanjing, median size is 50～80nm.
1, earlier to nano-TiO
2Carry out pre-treatment, with nano-TiO
2At room temperature immerse in the rare-earth modifier, soaked 5 hours, filter the back oven dry, obtain nano-TiO through the rare earth surface modification treatment
2The weight percentages of components of described rare-earth modifier is: cerium oxide 1.2%, ethanol 96%, ethylenediamine tetraacetic acid (EDTA) 0.4%, ammonium chloride 0.6%, nitric acid 0.5%, urea 1.3%.
2, the nano-TiO after will handling
2Mix with distilled water, be made into nano-TiO
2Weight percent be 10% solution, put into planetary ball mill ball milling 60min, rotating speed is 420r/min; With the nano-TiO that obtains behind the ball milling
2The baking oven of putting into 120 ℃ is fully dried, then with tetrafluoroethylene powder and nano-TiO
2Mix, carry out powerful mechanical stirring, in the mixed powder, nano-TiO
2Weight percent be 12%, the weight percent of tetrafluoroethylene is 88%.
3, mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 30MPa, and the time is 50 minutes, and pressurization and stress-relief process all slowly carry out.
4, the blank with above-mentioned compression moulding takes out gently, puts into muffle furnace, carries out sintering: slowly be warming up to about 330 ℃ earlier, and then be warming up to about 390 ℃ with 30 ℃/hour speed, be incubated 7 hours, make nano-TiO
2/ PTFE anti-wear composite material.
Above-mentioned gained nano TiO 2/ptfe composite is machined into the matrix material sample of 20mm * 10mm * 10mm, and record on the M-2000 friction wear testing machine: frictional coefficient is 0.21, and the specific wear rate is 1.12 * 10-14m3/N.m.
Recording its tensile strength according to the GB1040-79 standard is 28.4MPa.
Recording its flexural strength according to the GB/T9341-2000 standard is 49.5MPa.
Claims (3)
1, a kind of rare earth modified nano TiO
2/ ptfe composite preparation method is characterized in that comprising the steps:
1) with nano-TiO
2Immerse in the rare-earth modifier and soaked 2～5 hours, filter the back oven dry; The weight percentages of components of described rare-earth modifier is: rare earth compound 0.2～2.3%, ethanol 93.6～99.34%, ethylenediamine tetraacetic acid (EDTA) 0.03～0.7%, ammonium chloride 0.2～1%, nitric acid 0.03～0.6%, urea 0.2～1.8%;
2) nano-TiO after will handling
2Mix with distilled water, be made into nano-TiO
2Weight percent be 1～10% solution, put into planetary ball mill ball milling 15～65min, rotating speed is 120～550r/min; With the nano-TiO behind the ball milling
2After putting into the abundant oven dry of baking oven, carry out mechanical blending with the tetrafluoroethylene powder, the control nano-TiO
2Weight percent be 3～15% of mixed powder;
3) mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 30～40MPa, and the time is 30～50 minutes, and pressurization and stress-relief process all slowly carry out;
4) blank with above-mentioned compression moulding takes out gently, puts into muffle furnace, carries out sintering: slowly be warming up to 320～330 ℃ earlier, and then be warming up to 390 ℃ with 30 ℃/hour speed, be incubated 6～7 hours, obtain nano-TiO
2/ ptfe composite.
2,, it is characterized in that described rare earth compound is Cerium II Chloride, lanthanum trioxide, cerium oxide or Lanthanum trichloride according to the rare earth modified nano TiO2/ ptfe composite preparation method of claim 1.
3, according to the rare earth modified nano TiO of claim 1
2/ ptfe composite preparation method is characterized in that described tetrafluoroethylene is for the employing suspension polymerization and through the broken tetrafluoroethylene powder that forms of fine powder.
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| CN200910055617A CN101629004A (en) | 2009-07-30 | 2009-07-30 | Preparation method of rare earth modified nano TiO2/polytetrafluoroethylene composite |
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|---|---|---|---|
| CN200910055617A CN101629004A (en) | 2009-07-30 | 2009-07-30 | Preparation method of rare earth modified nano TiO2/polytetrafluoroethylene composite |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103100425A (en) * | 2013-01-16 | 2013-05-15 | 华南师范大学 | Method for weaving net composite catalytic material from nanometer titania and polytetrafluoroethylene in mixing manner, and application of net composite catalytic material |
| CN104479266A (en) * | 2014-12-26 | 2015-04-01 | 天津滨浦生产力促进有限公司 | Surface modification method of inorganic nanoparticles as well as polytetrafluoroethylene/inorganic nanoparticle composite material |
| CN105385056A (en) * | 2015-12-29 | 2016-03-09 | 南京大学 | Biological bactericidal plastic |
| CN106391091A (en) * | 2016-11-11 | 2017-02-15 | 江西德弘新材料有限公司 | Visible-light responsible photocatalyst and preparation method thereof |
| CN106496636A (en) * | 2016-10-24 | 2017-03-15 | 天津城建大学 | A kind of waste stone dust surface modifying method based on wet grinding |
| CN106633543A (en) * | 2017-01-06 | 2017-05-10 | 南京肯特复合材料股份有限公司 | Nanometer TiO2-modified polytrifluoroethylene and preparation method thereof |
| US9881714B2 (en) | 2014-06-19 | 2018-01-30 | Saint-Gobain Performance Plastics Corporation | Laser-markable insulation material for wire or cable assemblies |
| US10256009B2 (en) | 2014-06-19 | 2019-04-09 | Saint-Gobain Performance Plastics Corporation | Laser-markable insulation material for wire or cable assemblies |
| CN111393875A (en) * | 2020-03-30 | 2020-07-10 | 内蒙古航天红峡化工有限公司 | Preparation method of titanium dioxide coated rare earth base pearlescent pigment |
-
2009
- 2009-07-30 CN CN200910055617A patent/CN101629004A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103100425A (en) * | 2013-01-16 | 2013-05-15 | 华南师范大学 | Method for weaving net composite catalytic material from nanometer titania and polytetrafluoroethylene in mixing manner, and application of net composite catalytic material |
| US9881714B2 (en) | 2014-06-19 | 2018-01-30 | Saint-Gobain Performance Plastics Corporation | Laser-markable insulation material for wire or cable assemblies |
| US10256009B2 (en) | 2014-06-19 | 2019-04-09 | Saint-Gobain Performance Plastics Corporation | Laser-markable insulation material for wire or cable assemblies |
| CN104479266A (en) * | 2014-12-26 | 2015-04-01 | 天津滨浦生产力促进有限公司 | Surface modification method of inorganic nanoparticles as well as polytetrafluoroethylene/inorganic nanoparticle composite material |
| CN105385056A (en) * | 2015-12-29 | 2016-03-09 | 南京大学 | Biological bactericidal plastic |
| CN106496636A (en) * | 2016-10-24 | 2017-03-15 | 天津城建大学 | A kind of waste stone dust surface modifying method based on wet grinding |
| CN106391091A (en) * | 2016-11-11 | 2017-02-15 | 江西德弘新材料有限公司 | Visible-light responsible photocatalyst and preparation method thereof |
| CN106633543A (en) * | 2017-01-06 | 2017-05-10 | 南京肯特复合材料股份有限公司 | Nanometer TiO2-modified polytrifluoroethylene and preparation method thereof |
| CN111393875A (en) * | 2020-03-30 | 2020-07-10 | 内蒙古航天红峡化工有限公司 | Preparation method of titanium dioxide coated rare earth base pearlescent pigment |
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Open date: 20100120 |